反应详情

A mechanically stirred MeOH (3.8 L) suspension containing 1-[4-phenylmethoxy-3-nitrophenyl]ethanone (76.5 g, 282 mmol) was degassed with argon for 40 minutes at ~10° C. prior to addition of PtO2 (2.34 g, 10 mmol). Hydrogen was sparged into the reaction mixture at 8° C. to 10° C. via a subsurface gas inlet. After 8 hours, the completed reaction was degassed with Ar while being warmed to ~15° C., diluted with CHCl3 (250 mL) and filtered. The filtrate was stripped to give 70 g crude product which, after trituration for ten minutes with i-PrOH (450 mL) at 60° C., yielded 57.4 (84%) of the title compound.

1. customwas degassed with argon for 40 minutes at ~10° C.
2. customHydrogen was sparged into the reaction mixture at 8° C. to 10° C. via a subsurface gas inlet
3. customthe completed reaction
4. customwas degassed with Ar
5. temperaturewhile being warmed to ~15° C.
6. additiondiluted with CHCl3 (250 mL)
7. filtrationfiltered
8. customto give 70 g crude product which